CN102120021B - Detection method of concentrated pills for treating hyperplastic disease of breast - Google Patents
Detection method of concentrated pills for treating hyperplastic disease of breast Download PDFInfo
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Abstract
The invention discloses a detection method of concentrated pills for treating hyperplastic disease of breast, comprising five steps as follows: character examination, identification, routine pill examination, extract examination and content measurement. The formula of the concentrated pills comprises 125g of radix bupleuri, 125g of rhizoma cyperi, 83.4g of rhubarb (baked with wine), 83.4g of pericarpium citri reticulatae viride, 83.4g of ligusticum wallichii, 83.4g of curcuma zedoary, 83.4 g of ground beetle, 83.4g of thunberg fritillary bulb, 125g of Angelica sinensis, 125g of radix paeoniae alba and 83.4g of cowherb seed. The detection method is in favor of ensuring the quality of finished concentrated pills.
Description
Technical field
The invention belongs to technical field of traditional Chinese medicines, specifically relate to a kind of detection method of treating the concentrated pill of cyclomastopathy.
Background technology
Cyclomastopathy is common women's surgical disease, and its incidence of disease is high, has a strong impact on numerous women's physical and mental health, and this disease has the danger of the breast cancer of developing into.Thereby the active treatment cyclomastopathy, improve the WomanHealth level, reduce canceration rate and have very great significance.Modern medicine thinks, cyclomastopathy be because of endocrine dysfunction, ovarian dysfunction, cause body inner estrogen level to increase or increased activity, due to progesterone level descends.Obvious for the heavier or local tubercle of proliferation of mammary gland pain, the tangible patient of tenderness, clinical versatility hormonotherapy and endocrinotherapy.Like progesterone, red that azoles, TAM, bromocriptine etc.With the said method treatment, though curative effect is good, spinoff is bigger, and price is expensive, can not adhere to treatment for a long time, and pain recurrence after the drug withdrawal, lump increases, and finally still need continue treatment---excision.Especially sex hormone may further disturb the balance between the human hormone after using, and increases the possibility of canceration.In sum, this disease of modern medicine treatment is main with operation at present, and medicine is auxilliary.No matter be excision, drug therapy, have all that expense is high, spinoff is obvious, wound face is big, a shortcoming such as easy recurrence after operation or the drug withdrawal.Therefore doctor trained in Western medicine does not still have desirable solution route and methods of treatment to this disease.
Fibroid also is gynaecology's common disease, and doctor trained in Western medicine often adopts operative treatment, and myomata patient hysterectomizes before menopause.Even the reservation ovary often causes occurring ahead of time of climacteric syndrome, coronary heart disease and osteoporosis, and the overwhelming majority is carried out myomata and is rejected the art patient and can recur in a short time.Though treatment fibroid common chemical medicine can dwindle the myomata volume in short-term at present; Suppress uterine hemorrhage; But can not control the growth of myomata and new myomata occurs; And after using the medicine of these antagonism estrogen and progestational hormone, be easy to generate the low estrogen level, thereby bring out amenorrhoea, climacteric syndrome and osteoporosis etc.
In traditional Chinese medicine belonging fibroid symptoms refer, stone disease category." treatise on blood trouble " cloud: " fibroid be blood circulating out of vessels and good blood be not harmonious be the meaning hemostasis.With the passing of time then become disease ".This disease is because disorder of qi and blood, depressed rage impairing the liver, stagnation of QI due to depression of the liver accumulate in phlegm is wet, and the stasis of blood stagnates and forms long-pending piece, and liver kidney two void are due to the Chong and Ren channel disorder; Imbalance of yin and yang, liver-qi depression, kidney qi is not changed, and causes functional activity of QI being not smooth then, and qi depression to blood stasis is amassed and is formed note of the ancient Chinese disease.Fibroid mainly is visceral dysfunction, qi and blood discord so that blood stasis retardance, stay and tie to gather and form, and total interpretation of the cause, onset and process of an illness and hemostasis are inseparable.
The many methods of this disease of Chinese medicine with dispersing stagnated hepatoqi, the promoting flow of qi and blood circulation, broken stasis of blood reducing phlegm and resolving masses.Using qi-activating drug clinically is many with Ligusticum wallichii, rhizoma cyperi, Fructus Aurantii etc.; Drug for invigorating blood circulation and eliminating stasis is used peach kernel, safflower, the seed of cowherb etc. more; The dispersing stagnated hepatoqi medicine is used radix bupleuri, root tuber of aromatic turmeric etc. more; Apophlegmatisant is main with fritillaria thunbergii, marine alga, kelp then.The myomata tissue can not only controlled and dwindle to Chinese medicine aspect the treatment fibroid, comprehensive adjustment human hormone's level, and can improve clinical symptoms such as irregular menstruation, leukorrhea, the soreness of waist, late result is remarkable.Its effect many with improve microcirculation, to adjust body sex hormone level etc. relevant.At present, mainly contain guizhi fuling pill/capsule, palace knurl capsule for eliminating, Radix Et Rhizoma Rhei et Eupolyphaga Seu Steleophaga Pilulae and be used to treat fibroid, but still lack anti-fibroid determined curative effect, Chinese patent drug that safety coefficient is high.
Summary of the invention
The object of the invention provides a kind of detection method of treating the concentrated pill of cyclomastopathy, helps guaranteeing the quality of finished product.
The present invention treats the concentrated pill of cyclomastopathy and is made up of 11 flavor Chinese medicines, and concrete prescription is:
Radix bupleuri 125g, rhizoma cyperi 125g, rheum officinale (wine is processed) 83.4g, rascal 83.4g, Ligusticum wallichii 83.4g, curcuma zedoary 83.4g, ground bettle 83.4g, fritillaria thunbergii 83.4g, Radix Angelicae Sinensis 125g, root of herbaceous peony 125g, seed of cowherb 83.4g process 1000 balls.
Concrete preparation method:
The prepared RADIX ET RHIZOMA RHEI with wine of getting recipe quantity 1/2nd amounts is ground into fine powder, and is subsequent use.
Fritillaria thunbergii, the seed of cowherb add 5 times of amounts of 70% ethanol, refluxing extraction 2 times, and each 2 hours, filter, merging filtrate left standstill 16 hours, filtered, and filtrate recycling ethanol also is condensed into cream clearly, and is subsequent use.
Rhizoma cyperi, rascal, Ligusticum wallichii, curcuma zedoary and Radix Angelicae Sinensis steam distillation 6 hours extract volatile oil, and the WS after the distillation filters, and subsequent use, volatile oil is used the beta-schardinger dextrin-inclusion, the inclusion complex low temperature drying.
All the other four flavors such as remaining prepared RADIX ET RHIZOMA RHEI with wine add 10 times of amounts of water respectively, decoct each 1 hour 3 times; Filter, the WS after merging filtrate and the above-mentioned distillation, being concentrated into relative density is 1.05～1.10 (50 ℃); Left standstill 16 hours, centrifugal (2500 rev/mins) are got supernatant concentration and are become clear cream; Mix continued with the clear cream of above-mentioned alcohol extracting and be concentrated into the clear cream that relative density is 1.15～1.20 (50 ℃), get the clear cream spray drying about 90%, all the other clear cream continue to be concentrated into the thick paste of 1.35～1.38 (50 ℃); After spray dried powder and an amount of prepared RADIX ET RHIZOMA RHEI with wine fine powder, beta-cyclo dextrin included compound mixed, add an amount of dextrin mixing, close with the ethanol of 55%～75% concentration of 9～12% mixed powder amounts and stick together, mould and process pill; Get residue prepared RADIX ET RHIZOMA RHEI with wine fine powder again, an amount of thick paste is round as a ball with ball, drying is with residue thick paste, an amount of talcum powder and activated charcoal dressing; 1000 balls are processed in the insect wax polishing, promptly get.
This medicine is a compound Chinese medicinal preparation, and its prescription does not have openly with the preparation method before this, and the control method of its quality is not appeared in the newspapers.
Technical scheme of the present invention is:
The present invention treats the detection method of the concentrated pill of cyclomastopathy: comprise proterties, extract inspection, discriminating, pill routine inspection, 5 steps of assay, be specially:
A, proterties are: these article are black charcoal clothing condensed pill, and the ball core is a pitchy; Gas fragrance, little salty hardship of distinguishing the flavor of.
B, extract inspection are: get the about 4g of these article under the weight differential item, and porphyrize, the accurate title, decide, and puts in the conical flask, adds methyl alcohol l00ml, close plug; Claim to decide weight, put in the water-bath and refluxed 1 hour, be placed to room temperature, claim again to decide weight, supply the weight that subtracts mistake, shake up with methyl alcohol; Filter, discard filtrating just, precision is measured subsequent filtrate 50ml, and evaporate to dryness, residue add l0% sodium hydroxide solution 5ml makes dissolving, and is transferred in the separating funnel; Add water 25ml washing evaporating dish, washing lotion is incorporated in the same separating funnel, shakes up, and extracts 4 times with water saturated normal butyl alcohol, and each 30ml merges n-butanol extracting liquid; Add water washing 2 times, each 40ml discards water liquid, and normal butyl alcohol liquid is put in the evaporating dish that is dried to constant weight, behind evaporate to dryness in the water-bath; In 105 ℃ of dryings 3 hours, put in the exsiccator cooling 30 minutes, accurately rapidly claim decide weight, calculating promptly gets; These article contain the normal butyl alcohol extract must not be less than 1.2%;
C, discriminating are:
(1)
The thin-layer chromatography of radix bupleuri is differentiated:Get the normal butyl alcohol extract under the extract inspection item, add methyl alcohol 5ml and make dissolving, as need testing solution; Other gets radix bupleuri control medicinal material 0.5g, adds methyl alcohol 20ml sonicated 20 minutes, filters, and filtrating is concentrated into about 5ml, as control medicinal material solution.Get saikoside a reference substance again, add methyl alcohol and process the solution that every lml contains 0.5 mg, as reference substance solution; According to thin-layered chromatography; Each 5 μ l of above-mentioned three kinds of solution are drawn in test, put respectively on same silica gel g thin-layer plate; With ethyl acetate, alcohol and water 8:2:1 is developping agent, launches, and takes out; Dry, spray is with 40% sulfuric acid solution of 2% paradime thylaminobenzaldehyde, and it is clear to be heated to the spot colour developing at 60 ℃; Put under daylight and ultraviolet lamp 365 nm and inspect in the test sample chromatogram, with control medicinal material and the corresponding position of reference substance chromatogram on, show the spot or the fluorescence spot of same color
(2)
The thin-layer chromatography of rhizoma cyperi is differentiated:These article of getting 10g, porphyrize is put at the bottom of the garden in the flask; Add water 250ml, connect volatile oil determination apparatus and reflux condensing tube, add 2ml ethyl acetate again; Refluxed 10 minutes; Be placed to room temperature, get ethyl acetate layer and get α-cyperolone in addition, add ethyl acetate and process solution that every 1m1 contains lmg as reference substance solution as need testing solution.According to the thin-layered chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica GF254 thin layer plate, be developping agent with toluene-ethyl acetate-glacial acetic acid 92:5:5, launch, take out, dry, put under ultraviolet lamp 254 nm and inspect.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color; Spray is placed a moment with the dinitrophenylhydrazine test solution, and spot fades to orange red;
(3)
The thin-layer chromatography of rheum officinale is differentiated:These article of getting 0.3g, porphyrize adds methyl alcohol 20m1, and sonicated 15 minutes filters; Get filtrating 5m1, evaporate to dryness, residue add water 10ml makes dissolving, adds hydrochloric acid 1ml again; Reflux 30 minutes, cooling immediately divides 2 joltings to extract with ether, each 20m1; Merge ether solution, evaporate to dryness, residue add methenyl choloride 1m1 makes dissolving, as need testing solution; Other gets rheum officinale control medicinal material 0.1g, shines medicinal material solution in pairs with legal system; Get the Rhein reference substance again, add methyl alcohol and process the solution that every 1m1 contains 1mg, as reference substance solution; According to the thin-layered chromatography test, draw each 5 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate; Upper solution with sherwood oil (30～60 ℃)-ethyl formate-formic acid 15:5:1 is a developping agent, launches, and takes out; Dry, put under ultraviolet lamp 365 nm and inspect; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show five identical orange-yellow fluorescence principal spots; With the corresponding position of reference substance chromatogram on, show identical orange-yellow fluorescence spot, put in the ammonia steam smoked after, spot becomes redness;
(4)
The thin-layer chromatography of rascal is differentiated:These article of getting 2g, porphyrize adds methyl alcohol 20ml, and reflux 20 minutes filters; Get filtrating 10ml, evaporate to dryness, residue add water 2ml makes dissolving, through D10l macroporous adsorptive resins internal diameter 1.5cm, long 9cm; The post upper end adds the 1g neutral alumina, earlier with water 100m1 wash-out, discards, again with 2% pyridinemethanol 50m1 wash-out; Collect eluent, evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as need testing solution.Other gets the aurantiamarin reference substance, adds methyl alcohol and processes saturated solution, as reference substance solution; According to thin-layered chromatography; Each 2 μ l of above-mentioned two kinds of solution are drawn in test, put respectively in same with silica gel g thin-layer plate on, be developping agent with ethyl acetate-methanol-water 100:27:13; Exhibition is taken out to about 3cm, dries; Upper solution with toluene-ethyl acetate-formic acid-water 20:10:1:1 is a developping agent again, and exhibition is taken out to about 8cm; Dry, spray is put under the ultraviolet lamp 365nm and is inspected with the aluminium choride test solution; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the fluorescence spot of same color;
(5) Zhejiang
The thin-layer chromatography of the bulb of fritillary is differentiated:These article of getting 10g, porphyrize adds strong ammonia solution 2ml and methenyl choloride 50m1, and placement is spent the night, and filters; The filtrating evaporate to dryness, residue adds ethanol lml makes dissolving, admixes a little neutral alumina, mixes drying in the water-bath thoroughly; Be added on the neutral alumina post (100-200 order, 2g, the about 15mm of internal diameter), with ethanol 50ml wash-out; Collect eluent, evaporate to dryness, residue add ethanol lml makes dissolving, as need testing solution.Other gets the peimine reference substance, adds ethanol and processes the solution that every lml contains 2mg, as reference substance solution.According to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B); Reference substance solution 2 μ l, need testing solution 10 μ l are drawn in test, put respectively on same silica gel g thin-layer plate, and be developping agent with ethyl acetate-methyl alcohol-strong ammonia solution 17:2:1, launch, take out, to dry, spray is with rare bismuth potassium iodide test solution; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color;
(6)
The thin-layer chromatography of the root of herbaceous peony is differentiated:These article of getting 2g, porphyrize adds methyl alcohol 20ml, and reflux 20 minutes filters; Get filtrating l0ml, evaporate to dryness, residue add water 2ml makes dissolving, through D101 macroporous adsorptive resins internal diameter 1.5cm, long 9cm; The post upper end adds the lg neutral alumina, earlier with water l00ml wash-out, discards, again with 2% pyridinemethanol 50ml wash-out; Collect eluent, evaporate to dryness, residue add methyl alcohol lml makes dissolving, as need testing solution.Other gets the Paeoniflorin reference substance, adds ethanol and processes the solution that every lml contains lmg, as reference substance solution; According to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate; With methenyl choloride-ethyl acetate-methyl alcohol-formic acid 40:5:10:0.2 is developping agent; Launch, take out, dry; Spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear to be heated to the spot colour developing.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color;
D, pill routine inspection do
:Should meet each item regulation relevant under the Chinese Pharmacopoeia pill item;
E, assay
Chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filling agent; With methanol-water-glacial acetic acid 75:25:1 is moving phase; Detect wavelength 254nm; Number of theoretical plate calculates by the archen peak should be not less than 3000;
The preparation of reference substance solution: it is an amount of that precision takes by weighing aloe-emodin, Rhein, archen, Chrysophanol, Physcion reference substance; Adding methyl alcohol processes every lml respectively and contains each 150 μ g of Rhein, archen, Chrysophanol, the solution of aloe-emodin, each 75 μ g of Physcion; Precision is measured each 2ml of above-mentioned reference substance solution respectively, and mixing promptly gets every lml and contains Rhein, archen, each 30 μ g of Chrysophanol, aloe-emodin, each 15 μ g of Physcion;
The preparation of need testing solution: get these article under the weight differential item, porphyrize is got about 0.5g, and accurate the title decides, and puts in the tool plug conical flask, the accurate methyl alcohol 25ml that adds; Claim decide weight, reflux 30 minutes is put coldly, and weight decided in title again, supplies with methyl alcohol to subtract weight loss, shakes up; Filter, precision is measured subsequent filtrate 10ml, puts in the 50ml flask, flings to methyl alcohol, adds water 10ml, hydrochloric acid lml; Reflux 30 minutes, cooling immediately, and be transferred in the separating funnel, with a small amount of methenyl choloride washing container, incorporate in the separating funnel, extract 5 times with methenyl choloride; Each 30ml merges methenyl choloride liquid, with water 50ml washing once, discards water liquid, methenyl choloride liquid evaporate to dryness; Residue adds methyl alcohol and quantitatively is transferred in the 10ml measuring bottle, and is diluted to scale, shakes up, and filters, and promptly gets;
Determination method: accurate respectively above-mentioned reference substance solution and each 5 μ 1 of need testing solution of drawing, inject liquid chromatograph, measure, promptly get;
The every ball of these article contains prepared RADIX ET RHIZOMA RHEI with wine with aloe-emodin C
15H
10O
5, Rhein C
15H
80
6, archen C
15H
100
5, Chrysophanol C
15H
10O
4With Physcion C
16H
12O
5The total amount meter, must not be less than 0.6mg.
Advantage of the present invention is this medicine have been set up the detection method of the higher quality that can guarantee finished product.Because the contained flavour of a drug of these article are more; Complicated component; Detection method gropes just to set up through test of many times, and except that the routine inspection item of pill, the extract content of having set up monarch drug in a prescription radix bupleuri is measured, the high performance liquid chromatogram assay of ministerial drug rheum officinale; Set up the thin-layer chromatography of radix bupleuri, rhizoma cyperi, rheum officinale, rascal, fritillaria thunbergii, Chinese herbaceous peony 6 flavor Chinese medicines and differentiated, differentiated that flavour of a drug account for more than 50% of whole Chinese medicines.This detection method standard is higher, and its each step is inseparable, can guarantee the purpose of end product quality fully.
Embodiment
Below in conjunction with embodiment the present invention is further described:
Embodiment one: the preparation of concentrated pill
The concentrated pill prescription is: radix bupleuri 125g, rhizoma cyperi 125g, rheum officinale (wine is processed) 83.4g, rascal 83.4g, Ligusticum wallichii 83.4g, curcuma zedoary 83.4g, ground bettle 83.4g, fritillaria thunbergii 83.4g, Radix Angelicae Sinensis 125g, root of herbaceous peony 125g, seed of cowherb 83.4g, process 1000 balls.
The prepared RADIX ET RHIZOMA RHEI with wine of getting recipe quantity 1/2nd amounts is ground into fine powder, and is subsequent use.
Fritillaria thunbergii, the seed of cowherb add 5 times of amounts of 70% ethanol, refluxing extraction 2 times, and each 2 hours, filter, merging filtrate left standstill 16 hours, filtered, and filtrate recycling ethanol also is condensed into cream clearly, and is subsequent use.
Rhizoma cyperi, rascal, Ligusticum wallichii, curcuma zedoary and Radix Angelicae Sinensis steam distillation 6 hours extract volatile oil, and the WS after the distillation filters, and subsequent use, volatile oil is used the beta-schardinger dextrin-inclusion, the inclusion complex low temperature drying.
All the other four flavors such as remaining prepared RADIX ET RHIZOMA RHEI with wine add 10 times of amounts of water respectively, decoct each 1 hour 3 times; Filter, the WS after merging filtrate and the above-mentioned distillation, being concentrated into relative density is 1.05～1.10 (50 ℃); Left standstill 16 hours, centrifugal (2500 rev/mins) are got supernatant concentration and are become clear cream; Mix continued with the clear cream of above-mentioned alcohol extracting and be concentrated into the clear cream that relative density is 1.15～1.20 (50 ℃), get the clear cream spray drying about 90%, all the other clear cream continue to be concentrated into the thick paste of 1.35～1.38 (50 ℃); After spray dried powder and an amount of prepared RADIX ET RHIZOMA RHEI with wine fine powder, beta-cyclo dextrin included compound mixed, add an amount of dextrin mixing, close with the ethanol of 55%～75% concentration of 9～12% mixed powder amounts and stick together, mould and process pill; Get residue prepared RADIX ET RHIZOMA RHEI with wine fine powder again, an amount of thick paste is round as a ball with ball, drying is with residue thick paste, an amount of talcum powder and activated charcoal dressing; 1000 balls are processed in the insect wax polishing, promptly get.
The condensed pill that said method makes (to call condensed pill in the following text) is to the influence (result sees table 1) of mammary gland volume and mammary gland weight
Visible by table 1; The model group rabbit proliferation of mammary gland; The mammary gland volume obviously increases, and mammary gland weight obviously increases: with model group relatively, condensed pill 4g crude drug/kg, 2g crude drug/kg dose groups rabbit mammary gland volume all obviously reduce (P < O.05); Mammary gland weight also all obviously alleviates (P < O.05); Condensed pill 1g crude drug/>kg dose groups rabbit mammary gland volume, mammary gland weight and model group be no significant difference relatively all: with model group relatively, newborn disease spirit groups of grains rabbit mammary gland volume obviously reduces (P < O.05), mammary gland weight also obviously alleviates (P < O.05)).
Table 1. condensed pill to the influence of mammary gland volume and mammary gland weight (
± SD, n=8)
Annotate: compare * p < O.05 with model group
1. condensed pill is observed down the mirror of breast tissue influence
Rabbit breast tissue mirror is observed down: normal control group rabbit mammary gland does not have proliferative lesion, and leaflet is not obvious, and acinus is few, and fat and connective tissue are more, and the gland catheter lumen does not have expansion, is in the quiescent stage state; The model group rabbit proliferation of mammary gland is diffusivity, and mammary gland acinus and leaflet number significantly increase, and alveolar lumen and gland catheter lumen are obviously expanded, the cell that alveolar lumen includes secretion and comes off, and a matter reduces (seeing table 2).Condensed pill 4g crude drug/kg, 2g crude drug/kg dose groups and the above-mentioned variation of newborn disease spirit groups of grains breast tissue all have clear improvement, and condensed pill lg crude drug/above-mentioned variation of kg dose groups breast tissue does not have obviously and improves (seeing table 3).Compare with model group; Condensed pill 4g crude drug/kg, 2g crude drug/kg dose groups lobule of mammary gland number, mammary gland acinus number average obviously reduce (P < O.05～0.01); Condensed pill 4g crude drug/>kg dose groups alveolar lumen diameter has the trend of reducing, and condensed pill lg crude drug/kg dose groups rabbit lobule of mammary gland number, acinus number and alveolar lumen diameter and model group be no significant difference relatively all; Compare with model group, the also all obviously minimizings of the clever groups of grains rabbit of newborn disease lobule of mammary gland number, mammary gland acinus number (P O.05); Gland conduit diameter of three dose groups of condensed pill and newborn disease spirit groups of grains rabbit and model group be no significant difference relatively all.
Table 2. condensed pill to the influence of leaflet, acinus and gland conduit (
± SD, n=8)
Annotate: with model group relatively * p 0.05, * * p < 0.01
Embodiment two:The detection method of the concentrated pill of treatment cyclomastopathy may further comprise the steps, and is specially
:
A,Proterties: being described as these article by the virtual condition of big production sample is black charcoal clothing condensed pill, and the ball core is a pitchy; Gas fragrance, little salty hardship of distinguishing the flavor of.
,The extract inspection is: get the about 4g of these article under the weight differential item, and porphyrize, the accurate title, decide, and puts in the conical flask, adds methyl alcohol l00ml, close plug; Claim to decide weight, put in the water-bath and refluxed 1 hour, be placed to room temperature, claim again to decide weight, supply the weight that subtracts mistake, shake up with methyl alcohol; Filter, discard filtrating just, precision is measured subsequent filtrate 50ml, and evaporate to dryness, residue add l0% sodium hydroxide solution 5ml makes dissolving, and is transferred in the separating funnel; Add water 25ml washing evaporating dish, washing lotion is incorporated in the same separating funnel, shakes up, and extracts 4 times with water saturated normal butyl alcohol, and each 30ml merges n-butanol extracting liquid; Add water washing 2 times, each 40ml discards water liquid, and normal butyl alcohol liquid is put in the evaporating dish that is dried to constant weight, behind evaporate to dryness in the water-bath; In 105 ℃ of dryings 3 hours, put in the exsiccator cooling 30 minutes, accurately rapidly claim decide weight, calculating promptly gets.These article contain the normal butyl alcohol extract all greater than 1.2%.
, differentiate that the thin-layer chromatography of (1) radix bupleuri differentiates
The preparation of reference substance: (identify institute available from Chinese pharmaceutical biological product, lot number is: 110777-200406), add methyl alcohol and process the solution that every lml contains 0.5mg, as reference substance solution to get saikoside a reference substance.(identify institute available from Chinese pharmaceutical biological product, lot number is: 120992-200705), add methyl alcohol 20ml sonicated 20 minutes, filter, filtrating is concentrated into about 5ml, as control medicinal material solution to get radix bupleuri control medicinal material 0.5g.
The preparation of test sample: get the normal butyl alcohol extract under the extract inspection item, add methyl alcohol 5ml and make dissolving, as need testing solution.
According to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, draw each 5 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate; With ethyl acetate, alcohol and water (8:2:1) is developping agent, launches, and takes out; Dry; Spray is with 40% sulfuric acid solution of 2% paradime thylaminobenzaldehyde, and it is clear to be heated to the spot colour developing at 60 ℃, puts under daylight and the ultraviolet lamp (365 nm) and inspects.In the test sample chromatogram, with control medicinal material and the corresponding position of reference substance chromatogram on, show the spot or the fluorescence spot of same color.
(2) thin-layer chromatography of rhizoma cyperi is differentiated
The preparation of reference substance: (identify institute available from Chinese pharmaceutical biological product, lot number is: 110748-200608), add ethyl acetate and process solution that every 1m1 contains lmg as reference substance solution to get α-cyperolone reference substance.
The preparation of test sample: get these article l0g, porphyrize is put at the bottom of the garden in the flask; Add water 250ml, connect volatile oil determination apparatus and reflux condensing tube (on analyzer, add water make be full of scale), add 2ml ethyl acetate again; Refluxed 10 minutes, and be placed to room temperature, get ethyl acetate layer as need testing solution.
Test according to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B); Drawing each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica GF254 thin layer plate, is developping agent with toluene-ethyl acetate-glacial acetic acid (92:5:5); Launch; Take out, dry, put under the ultraviolet lamp (254 nm) and inspect.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color; Spray is placed a moment with the dinitrophenylhydrazine test solution, and spot fades to orange red.
(3) thin-layer chromatography of rheum officinale is differentiated
The preparation of reference substance: (identify institute available from Chinese pharmaceutical biological product, lot number is: 110757-200206), add methyl alcohol and process the solution that every 1m1 contains 1mg, as reference substance solution to get the Rhein reference substance.(identify institute available from Chinese pharmaceutical biological product, lot number is: 121249-200402) 0.1g adds methyl alcohol 20m1, sonicated 15 minutes, filtration to get the rheum officinale control medicinal material; Get filtrating 5m1, evaporate to dryness, residue add water 10ml makes dissolving, adds hydrochloric acid 1ml again; Reflux 30 minutes, cooling immediately divides 2 joltings to extract with ether, each 20m1; Merge ether solution, evaporate to dryness, residue add methenyl choloride 1m1 makes dissolving, as the paired medicinal material solution that shines.
The preparation of test sample: get these article 0.3g, porphyrize adds methyl alcohol 20m1, and sonicated 15 minutes filters; Get filtrating 5m1, evaporate to dryness, residue add water 10ml makes dissolving, adds hydrochloric acid 1ml again; Reflux 30 minutes, cooling immediately divides 2 joltings to extract with ether, each 20m1; Merge ether solution, evaporate to dryness, residue add methenyl choloride 1m1 makes dissolving, as need testing solution.
Test according to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B); Drawing each 5 μ 1 of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, is developping agent with the upper solution of sherwood oil (30～60 ℃)-ethyl formate-formic acid (15:5:1); Launch; Take out, dry, put under the ultraviolet lamp (365nm) and inspect.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show five identical orange-yellow fluorescence principal spots; With the corresponding position of reference substance chromatogram on, show identical orange-yellow fluorescence spot, put in the ammonia steam smoked after, spot becomes redness.
(4) thin-layer chromatography of rascal is differentiated
The preparation of reference substance: (identify institute available from Chinese pharmaceutical biological product, lot number is: 110721-200613), add methyl alcohol and process saturated solution, as reference substance solution to get the aurantiamarin reference substance.
The preparation of test sample: get these article 2g, porphyrize adds methyl alcohol 20ml, and reflux 20 minutes filters; Get filtrating 10ml, evaporate to dryness, residue add water 2ml makes dissolving, through D101 macroporous adsorptive resins (internal diameter 1.5cm, long 9cm; The post upper end adds the 1g neutral alumina), earlier with water 100ml wash-out, discard, again with 2% pyridinemethanol 50m1 wash-out; Collect eluent, evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as need testing solution.
According to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, draw each 2 μ l of above-mentioned two kinds of solution, put respectively in same with silica gel g thin-layer plate on, be developping agent with ethyl acetate-methanol-water (100:27:13); Exhibition is taken out to about 3cm, dries; Upper solution with toluene-ethyl acetate-formic acid-water (20:10:1:1) is a developping agent again, and exhibition is taken out to about 8cm; Dry, spray is put under the ultraviolet lamp (365nm) and is inspected with the aluminium choride test solution.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the fluorescence spot of same color.
(5) thin-layer chromatography of fritillaria thunbergii is differentiated
The preparation of reference substance: (identify institute available from Chinese pharmaceutical biological product, lot number is: 110750-200608), add ethanol and process the solution that every lml contains 2mg, as reference substance solution to get the peimine reference substance.
The preparation of test sample: get these article 10g, porphyrize adds strong ammonia solution 2ml and methenyl choloride 50m1, and placement is spent the night, and filters; The filtrating evaporate to dryness, residue adds ethanol lml makes dissolving, admixes a little neutral alumina, mixes drying in the water-bath thoroughly; Be added on the neutral alumina post (100-200 order, 2g, the about 15mm of internal diameter), with ethanol 50ml wash-out; Collect eluent, evaporate to dryness, residue add ethanol lml makes dissolving, as need testing solution.
Test according to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B); Drawing reference substance solution 2 μ 1, need testing solution 10 μ l, put respectively on same silica gel g thin-layer plate, is developping agent with ethyl acetate-methyl alcohol-strong ammonia solution (17:2:1); Launch; Take out, dry, spray is with rare bismuth potassium iodide test solution.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color.
(6) thin-layer chromatography of the root of herbaceous peony is differentiated
The preparation of reference substance: (identify institute available from Chinese pharmaceutical biological product, lot number is: 110736-200833), add ethanol and process the solution that every lml contains lmg, as reference substance solution to get the Paeoniflorin reference substance.
The preparation of test sample: get these article 2g, porphyrize adds methyl alcohol 20ml, and reflux 20 minutes filters; Get filtrating l0ml, evaporate to dryness, residue add water 2ml makes dissolving, through D101 macroporous adsorptive resins (internal diameter 1.5cm, long 9cm; The post upper end adds the lg neutral alumina), earlier with water l00ml wash-out, discard, again with 2% pyridinemethanol 50ml wash-out; Collect eluent, evaporate to dryness, residue add methyl alcohol lml makes dissolving, as need testing solution.
According to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate; With methenyl choloride-ethyl acetate-methyl alcohol-formic acid (40:5:10:0.2) is developping agent; Launch, take out, dry; Spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear to be heated to the spot colour developing.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color.
D, pill routine inspection
:These article are condensed pill; Relevant regulations by under the condensed pill item in the Chinese Pharmacopoeia appendix I A pill detect; Comprise weight differential, content uniformity, moisture, dissolve scattered time limit, the checks such as mite, bacterial population, mould and saccharomycete, EHEC, coliform, detection of Salmonella of living, each item all meets the pharmacopeia regulation as a result.
, assay
(1) instrument and reagent
Instrument: Tianjin, island high performance liquid chromatograph (LC-20AT solvent delivery pump, SPD-10A UV-detector, N-2000 chromatographic work station; Tianjin, island CTO-10ASVP column oven).
Reagent: methyl alcohol is chromatographically pure; Ultrapure water; It is pure that all the other reagent are analysis; (aloe-emodin, Rhein, archen, Chrysophanol, Physcion are that Nat'l Pharmaceutical & Biological Products Control Institute provides to reference substance, supply assay usefulness, lot number: 110795-200806,110757-200206,110756-200110,110796-200716,110758-200611.
(2) chromatographic condition
Chromatographic column: Phenomenex Gemini 5 μ C18 110A (250 * 4.60mm, 5 micron); Column temperature: 35 ℃; Moving phase: methanol-water-glacial acetic acid (75:25:1); Flow velocity: 1.0 ml/min; Detect wavelength 254nm.Sample size 5 μ 1.Under this chromatographic condition, reference substance chromatographic peak and adjacent peak reach baseline separation, and degree of separation is greater than 1.5, and number of theoretical plate calculates by the archen peak should be not less than 3000.
(3) preparation of reference substance solution
It is an amount of that precision takes by weighing aloe-emodin, Rhein, archen, Chrysophanol, Physcion reference substance, adds methyl alcohol and process every lml respectively and contain Rhein, archen, each 150 μ g of Chrysophanol, the solution of aloe-emodin, each 75 μ g of Physcion; Precision is measured each 2ml of above-mentioned reference substance solution respectively, and mixing promptly gets (every lml contains Rhein, archen, each 30 μ g of Chrysophanol, aloe-emodin, each 15 μ g of Physcion).
(4) preparation of need testing solution
Get these article under the weight differential item, porphyrize is got about 0.5g, and accurate the title decides, and puts in the tool plug conical flask, the accurate methyl alcohol 25ml that adds; Claim decide weight, reflux 30 minutes is put coldly, and weight decided in title again, supplies with methyl alcohol to subtract weight loss, shakes up; Filter, precision is measured subsequent filtrate 10ml, puts in the 50ml flask, flings to methyl alcohol, adds water 10ml, hydrochloric acid lml; Reflux 30 minutes, cooling immediately, and be transferred in the separating funnel, with a small amount of methenyl choloride washing container, incorporate in the separating funnel, extract 5 times with methenyl choloride; Each 30ml merges methenyl choloride liquid, with water 50ml washing once, discards water liquid, methenyl choloride liquid evaporate to dryness; Residue adds methyl alcohol and quantitatively is transferred in the 10ml measuring bottle, and is diluted to scale, shakes up, and filters, and promptly gets.
(5) determination method
Accurate respectively above-mentioned reference substance solution and each 5 μ 1 of need testing solution of drawing inject liquid chromatograph, measure, and promptly get.
The every ball of these article contains prepared RADIX ET RHIZOMA RHEI with wine with aloe-emodin (C
15H
10O
5), Rhein (C
15H
80
6), archen (C
15H
100
5), Chrysophanol (C
15H
10O
4) and Physcion (C
16H
12O
5) the total amount meter, must not be less than 0.6mg.By last method do to the mensuration result of 3 batches of products, 0.88,0.87,0.88 mg/ ball, all up to specification.
Above-mentioned each step is as the ingredient of the detection method of this pill, interwoveness, and the finished product that meets above all inspections is specification product.
Claims (1)
1. a detection method of treating the concentrated pill of cyclomastopathy comprises proterties, extract inspection, discriminating, pill routine inspection, five steps of assay,
A, proterties are: these article are black charcoal clothing condensed pill, and the ball core is a pitchy; Gas fragrance, little salty hardship of distinguishing the flavor of;
B, extract inspection are: get the about 4g of these article under the weight differential item, and porphyrize, the accurate title, decide, and puts in the conical flask, adds methyl alcohol l00ml, close plug; Claim to decide weight, put in the water-bath and refluxed 1 hour, be placed to room temperature, claim again to decide weight, supply the weight that subtracts mistake, shake up with methyl alcohol; Filter, discard filtrating just, precision is measured subsequent filtrate 50ml, and evaporate to dryness, residue add l0% sodium hydroxide solution 5ml makes dissolving, and is transferred in the separating funnel; Add water 25ml washing evaporating dish, washing lotion is incorporated in the same separating funnel, shakes up, and extracts 4 times with water saturated normal butyl alcohol, and each 30ml merges n-butanol extracting liquid; Add water washing 2 times, each 40ml discards water liquid, and normal butyl alcohol liquid is put in the evaporating dish that is dried to constant weight, behind evaporate to dryness in the water-bath; In 105 ℃ of dryings 3 hours, put in the exsiccator cooling 30 minutes, accurately rapidly claim decide weight, calculating promptly gets; These article contain the normal butyl alcohol extract must not be less than 1.2%;
C, discriminating are:
(1)
The thin-layer chromatography of radix bupleuri is differentiated:Get the normal butyl alcohol extract under the extract inspection item, add methyl alcohol 5ml and make dissolving, as need testing solution; Other gets radix bupleuri control medicinal material 0.5g, adds methyl alcohol 20ml sonicated 20 minutes, filters, and filtrating is concentrated into about 5ml, as control medicinal material solution; Get saikoside a reference substance again, add methyl alcohol and process the solution that every lml contains 0.5 mg, as reference substance solution; According to thin-layered chromatography; Each 5 μ l of above-mentioned three kinds of solution are drawn in test, put respectively on same silica gel g thin-layer plate; With ethyl acetate, alcohol and water 8:2:1 is developping agent, launches, and takes out; Dry, spray is with 40% sulfuric acid solution of 2% paradime thylaminobenzaldehyde, and it is clear to be heated to the spot colour developing at 60 ℃; Put under daylight and ultraviolet lamp 365 nm and inspect in the test sample chromatogram, with control medicinal material and the corresponding position of reference substance chromatogram on, show the spot or the fluorescence spot of same color;
(2)
The thin-layer chromatography of rhizoma cyperi is differentiated:These article of getting 10g, porphyrize is put at the bottom of the garden in the flask; Add water 250ml, connect volatile oil determination apparatus and reflux condensing tube, add 2ml ethyl acetate again; Refluxed 10 minutes; Be placed to room temperature, get ethyl acetate layer and get α-cyperolone in addition, add ethyl acetate and process solution that every 1m1 contains lmg as reference substance solution as need testing solution; According to the thin-layered chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica GF254 thin layer plate, be developping agent with toluene-ethyl acetate-glacial acetic acid 92:5:5, launch, take out, dry, put under ultraviolet lamp 254 nm and inspect; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color; Spray is placed a moment with the dinitrophenylhydrazine test solution, and spot fades to orange red;
(3)
The thin-layer chromatography of rheum officinale is differentiated:These article of getting 0.3g, porphyrize adds methyl alcohol 20m1, and sonicated 15 minutes filters; Get filtrating 5m1, evaporate to dryness, residue add water 10ml makes dissolving, adds hydrochloric acid 1ml again; Reflux 30 minutes, cooling immediately divides 2 joltings to extract with ether, each 20m1; Merge ether solution, evaporate to dryness, residue add methenyl choloride 1m1 makes dissolving, as need testing solution; Other gets rheum officinale control medicinal material 0.1g, shines medicinal material solution in pairs with legal system; Get the Rhein reference substance again, add methyl alcohol and process the solution that every 1m1 contains 1mg, as reference substance solution; According to the thin-layered chromatography test, draw each 5 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate; Upper solution with 30～60 ℃ of sherwood oil-ethyl formates-formic acid 15:5:1 is a developping agent, launches, and takes out; Dry, put under ultraviolet lamp 365 nm and inspect; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show five identical orange-yellow fluorescence principal spots; With the corresponding position of reference substance chromatogram on, show identical orange-yellow fluorescence spot, put in the ammonia steam smoked after, spot becomes redness;
(4)
The thin-layer chromatography of rascal is differentiated:These article of getting 2g, porphyrize adds methyl alcohol 20ml, and reflux 20 minutes filters; Get filtrating 10ml, evaporate to dryness, residue add water 2ml makes dissolving, through D10l macroporous adsorptive resins internal diameter 1.5cm, long 9cm; The post upper end adds the 1g neutral alumina, earlier with water 100m1 wash-out, discards, again with 2% pyridinemethanol 50m1 wash-out; Collect eluent, evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as need testing solution; Other gets the aurantiamarin reference substance, adds methyl alcohol and processes saturated solution, as reference substance solution; According to thin-layered chromatography; Each 2 μ l of above-mentioned two kinds of solution are drawn in test, put respectively in same with silica gel g thin-layer plate on, be developping agent with ethyl acetate-methanol-water 100:27:13; Exhibition is taken out to about 3cm, dries; Upper solution with toluene-ethyl acetate-formic acid-water 20:10:1:1 is a developping agent again, and exhibition is taken out to about 8cm; Dry, spray is put under the ultraviolet lamp 365nm and is inspected with the aluminium choride test solution; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the fluorescence spot of same color;
(5) Zhejiang
The thin-layer chromatography of the bulb of fritillary is differentiated:These article of getting 10g, porphyrize adds strong ammonia solution 2ml and methenyl choloride 50m1, and placement is spent the night, and filters; The filtrating evaporate to dryness, residue adds ethanol lml makes dissolving, admixes a little neutral alumina, mixes drying in the water-bath thoroughly, is added on the neutral alumina post; The 100-200 order, 2g, the about 15mm of internal diameter is with ethanol 50ml wash-out; Collect eluent, evaporate to dryness, residue add ethanol lml makes dissolving, as need testing solution; Other gets the peimine reference substance, adds ethanol and processes the solution that every lml contains 2mg, as reference substance solution; According to thin-layered chromatography; Reference substance solution 2 μ l, need testing solution 10 μ l are drawn in test, put respectively on same silica gel g thin-layer plate, and be developping agent with ethyl acetate-methyl alcohol-strong ammonia solution 17:2:1, launch, take out, to dry, spray is with rare bismuth potassium iodide test solution; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color;
(6)
The thin-layer chromatography of the root of herbaceous peony is differentiated:These article of getting 2g, porphyrize adds methyl alcohol 20ml, and reflux 20 minutes filters; Get filtrating l0ml, evaporate to dryness, residue add water 2ml makes dissolving, through D101 macroporous adsorptive resins internal diameter 1.5cm, long 9cm; The post upper end adds the lg neutral alumina, earlier with water l00ml wash-out, discards, again with 2% pyridinemethanol 50ml wash-out; Collect eluent, evaporate to dryness, residue add methyl alcohol lml makes dissolving, as need testing solution; Other gets the Paeoniflorin reference substance, adds ethanol and processes the solution that every lml contains lmg, as reference substance solution; According to the thin-layered chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate; With methenyl choloride-ethyl acetate-methyl alcohol-formic acid 40:5:10:0.2 is developping agent, launches, and takes out; Dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear to be heated to spot colour developing; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color;
D, pill routine inspection do
:Should meet each item regulation relevant under the Chinese Pharmacopoeia pill item;
E, assay:
Chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filling agent; With methanol-water-glacial acetic acid 75:25:1 is moving phase; Detect wavelength 254nm; Number of theoretical plate calculates by the archen peak should be not less than 3000;
The preparation of reference substance solution: it is an amount of that precision takes by weighing aloe-emodin, Rhein, archen, Chrysophanol, Physcion reference substance; Adding methyl alcohol processes every lml respectively and contains each 150 μ g of Rhein, archen, Chrysophanol, the solution of aloe-emodin, each 75 μ g of Physcion; Precision is measured each 2ml of above-mentioned reference substance solution respectively, and mixing promptly gets every lml and contains Rhein, archen, each 30 μ g of Chrysophanol, aloe-emodin, each 15 μ g of Physcion;
The preparation of need testing solution: get these article under the weight differential item, porphyrize is got about 0.5g, and accurate the title decides, and puts in the tool plug conical flask, the accurate methyl alcohol 25ml that adds; Claim decide weight, reflux 30 minutes is put coldly, and weight decided in title again, supplies with methyl alcohol to subtract weight loss, shakes up; Filter, precision is measured subsequent filtrate 10ml, puts in the 50ml flask, flings to methyl alcohol, adds water 10ml, hydrochloric acid lml; Reflux 30 minutes, cooling immediately, and be transferred in the separating funnel, with a small amount of methenyl choloride washing container, incorporate in the separating funnel, extract 5 times with methenyl choloride; Each 30ml merges methenyl choloride liquid, with water 50ml washing once, discards water liquid, methenyl choloride liquid evaporate to dryness; Residue adds methyl alcohol and quantitatively is transferred in the 10ml measuring bottle, and is diluted to scale, shakes up, and filters, and promptly gets;
Determination method: accurate respectively above-mentioned reference substance solution and each 5 μ 1 of need testing solution of drawing, inject liquid chromatograph, measure, promptly get;
The every ball of these article contains prepared RADIX ET RHIZOMA RHEI with wine with aloe-emodin C
15H
10O
5, Rhein C
15H
80
6, archen C
15H
100
5, Chrysophanol C
15H
10O
4With Physcion C
16H
12O
5The total amount meter, must not be less than 0.6mg;
The concentrated pill of wherein said treatment cyclomastopathy is made up of 11 flavor Chinese medicines, and concrete prescription is:
Radix bupleuri 125g, rhizoma cyperi 125g, wine Radix Et Rhizoma Rhei (processed) 83.4g, rascal 83.4g, Ligusticum wallichii 83.4g, curcuma zedoary 83.4g, ground bettle 83.4g, fritillaria thunbergii 83.4g, Radix Angelicae Sinensis 125g, root of herbaceous peony 125g, seed of cowherb 83.4g process 1000 balls.
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| CN103399094A (en) * | 2013-07-30 | 2013-11-20 | 雷允上药业有限公司 | Fingerprint spectrum detection method of pills for treating hyperplasia of mammary glands |
| CN103356967A (en) * | 2013-07-30 | 2013-10-23 | 雷允上药业有限公司 | Chinese herbal compound extract with effect of resisting proliferation of mammary gland, and preparation method thereof |
| CN103558330B (en) * | 2013-10-08 | 2016-01-20 | 九芝堂股份有限公司 | A kind of TLC distinguish chromatographic process of Jianwei Yuyang preparation |
| CN104749312A (en) * | 2013-12-27 | 2015-07-01 | 天津中新药业集团股份有限公司乐仁堂制药厂 | Detection method for effective components in silky fowl tablet |
| CN106814157B (en) * | 2017-01-17 | 2018-11-20 | 广州浩意万医药科技有限公司 | The preparation method of green peel reference extract |
| CN110031588B (en) * | 2019-03-26 | 2021-02-09 | 浙江金大康动物保健品有限公司 | One-plate multi-medicine-taste rapid thin-layer identification method for livestock and poultry antiviral particles |
| CN112268968B (en) * | 2020-10-16 | 2022-05-10 | 山东步长神州制药有限公司 | Detection method of fingerprint spectrum of medicinal preparation |
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